Sulfurizing and leading unsaponifiable portions of degras



United States Patent SULFURIZING AND LEADING UNSAPONIFIABLE PORTIONS OF DEGRAS Conrad J. Sunde, Garden City, N. Y., assignor to N. I.

Malmstrom & Company, Brooklyn, N. Y., a copartnership No Drawing. Application April 2, 1949,

Serial No. 85,254 I 1 Claim. (Cl. 252-33.6)

The present invention relates to a process for sulfurizing the unsaponifiable portions of fatty and waxy mate rials, and more particularly to the sulfurizing of the unsaponifiable portions of wool grease .or lanolin, which is also known in the trade as degras.

It is among the objects of the present invention to provide a simple, inexpensive process for sulfurizing the unsaponifiable portions of fatty and waxy materials and particularly the unsaponifiable portions of wool grease or degras to give increased yields of highly sulfurized products with less conversion to undesirable by-products.

Another object is to provide a novel sulfurized product derived from the unsaponifiable portions of wool grease or degras which may be most effectively utilized as an additive for mineral oils and particularly lubricating oils, so that they may be used in high pressure lubricants and also generally in motor oils and other lubricating combinations.

Still further objects and advantages will appear in the more detailed description set forth below, it being understood, however, that this more detailed description is given by way of illustration and explanation only and not by way of limitation, since various changes therein may be made by those skilled in the art without departing from the scope and spirit of the present invention.

According to the present invention, it has been found most satisfactory first to disperse the unsaponifiable portions of lanolin, wool grease or degras in hydrocarbon, such as mineral or lubricating oil. This procedure is followed by stirring and heating to an elevated temperature of about 225 to 350 F.; then a dispersion of phosphorous pentasulfide in mineral oil is added to the dispersed unsaponifiable portions of the lanolin, wool grease or degras.

After maintaining this mixture at an elevated temperature for a period which may range from minutes to several hours, the mixture may be filtered and used as an additive or in any other connections.

If desired, as a last step, a heavy metal may be added in the form of a water soluble salt and a sulfurized, metallized, unsaponifiable fraction of lanolin or wool grease may thus be produced.

To give a specific example of the above procedure:

Example About 100 parts by weight of the unsaponifiable portion of lanolin, wool grease or degras are placed in 50 parts by weight of a suitable mineral oil, such as lubricating oil. I

The mixture is heated, with stirring, to 275 to 350 F., and preferably to 285 F.

A slurry of phosphorous pentasulfide (23 to 75 parts 2,710,836 Patented June 14, 1955 by weight) depending on the sulfur content desired in the final product, in 50 parts of mineral oil or lubricating oil is added in small portions during a period of approximately one-half hour.

The reaction mixture is maintained at a temperature of 280 to 300 F. during this addition. Since an exothermic reaction takes place, cooling may be necessary.

Stirring is continued after the addition is completed, and the reaction mixture is held at a temperature of 285 to 300 F. for an hour, after which it is separated from the sludge.

After cooling somewhat, a stream of air is passed through the mass for a period of 2 to 3 hours. During this period a temperature up to 240 F. is maintained.

One to two percent of a mixture of 9 parts of clay -to 1 part of charcoal is added. The mixture is then filtered.

It is often desirable to add heavy metal salts, such as lead, and this may be done by combining about 100 parts by weight of sulfurized, unsaponifiable portions of degras or lanolin with about 24 parts of lead acetate. Specifically, 100 parts by weight of sulfurized unsaponifiable portions of wool grease or degras are heated to approximately 200 F. A solution of 24 parts by weight of lead acetate in about 24 grams of water is added to the mixture. The mixture is then heated to about 200 to 210 F. for 45 minutes.

The acetic acid may be removed in a number of ways. For example, the product may be cooled and excess water added, followed by heating with a steam bath and stirring.

After cooling, the wash water may be decanted and after 7 three or four washings, the product may be dried at 212 F.

The residual acetic acid and water may also be removed,

Mercury Tin Iron Silver Copper Nickel Lead Cadmium In combination with the sulfurized, unsaponifiable portions of degras, it is also possible to utilize various alkyl and aryl thiophosphates or thiophosphites. Instead of phosphorous pentasulfide in addition thereto, it is also possible to use phosphorous sesquisulfide.

The embodiment of the invention shown and described herein is to be considered merely as illustrative, as the invention is susceptible to variations, modification and change within the spirit and scope of the appended claim.

Having now particularly described and ascertained the nature of the invention, and in what manner the same is to be performed, what is claimed is:

A process of sulfurizing and leading the unsaponifiable portions of degras which comprises dispersing 100 parts of the unsaponifiable portion of degras in 50 parts of a lubricating oil while heating with stirring to 275 to 300 F., adding a slurry of phosphorous pentasulfide in the amount of 23 to parts by weight dispersed in 50 parts by weight of lubricating oil over a period of one-half hour while maintaining a temperature of 280 to 300 F., passing a stream of air through the mixture for a period oi two to three hours while maintaining a temperature of about 240 F., and then combining 100 parts by weight of the mixture with about 24 parts by weight of lead acetate at a temperature of 200 to 210 F. for 45 minutes and blowing air through the mixture for about 45 minutes at 210 to 220 F. to remove residual water and acetic acid.

References Cited in the file of this patent UNITED STATES PATENTS Abramowitz Mar. 9, 1943 Williams et a1. May 1, 1945 Williams May 6, 1947 Musselman Apr. 20,1948 

